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Field emission properties from flexible field emitters using carbon nanotube film

Dong Hoon Shin, Seung Il Jung, Ki Nam Yun, Guohai Chen, Yoon-Ho Song, Yahachi Saito, William I. Milne, and
Cheol Jin Lee
Citation: Applied Physics Letters 105, 033110 (2014); doi: 10.1063/1.4891328
View online: http://dx.doi.org/10.1063/1.4891328
View Table of Contents: http://scitation.aip.org/content/aip/journal/apl/105/3?ver=pdfcov
Published by the AIP Publishing
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APPLIED PHYSICS LETTERS 105, 033110 (2014)

Field emission properties from flexible field emitters using carbon nanotube
film
Dong Hoon Shin,1,a) Seung Il Jung,1,a),b) Ki Nam Yun,1 Guohai Chen,2 Yoon-Ho Song,3
Yahachi Saito,4 William I. Milne,5 and Cheol Jin Lee1,c)
1

School of Electrical Engineering, Korea University, Seoul 136-713, South Korea


National Institute of Advanced Industrial Science and Technology (AIST), and Technology Research
Association for Single Wall Carbon Nanotubes (TASC), Tsukuba, Ibaraki 305-8565, Japan
3
Nano Electron-Source Creative Research Center, Creative and Challenging Research Division, Electronics
and Telecommunications Research Institute, Daejeon 305-700, South Korea
4
Department of Quantum Engineering, Graduate School of Engineering, Nagoya University,
Nagoya 464-8603, Japan
5
Electrical Engineering Division, Department of Engineering, Cambridge University,
Cambridge CB3 0FA, United Kingdom
2

(Received 17 April 2014; accepted 6 July 2014; published online 24 July 2014)
Flexible carbon nanotube (CNT) field emitters are fabricated using CNT films on polyethylene
terephthalate films. The flexible CNT emitters, which are made using double-walled CNTs, show
high emission performance and also indicate stable field emission properties under several bending
conditions. The flexible CNT emitters have a low turn-on field of about 0.82 V/lm and a high emission current density of about 2.0 mA/cm2 at an electric field of 1.6 V/lm. During stability tests, the
flexible CNT emitters initially degrade over the first 4 h but exhibit no further significant
degradation over the next 16 h testing while being continually bent. A flexible lamp made using the
C 2014
flexible CNT emitter displays uniform and bright emission patterns in a convex mode. V
AIP Publishing LLC. [http://dx.doi.org/10.1063/1.4891328]

Carbon nanotubes (CNTs) have been touted as one of


the most promising field emission materials due to their high
aspect ratio, high electrical conductivity, good thermal conductivity, and high chemical stability.16 There have been
many reports on various applications using CNT emitters.711 Most CNT based field emitters have been fabricated
on rigid substrates such as silicon substrates, glass substrates,
and metal substrates.1215 Recently, field emitters, especially
CNT based field emitters, fabricated on flexible substrates
have become of increasing interest1622 because they can be
used in diverse applications like bendable displays, roundshaped signage boards or three dimensional X-ray sources.
The key issue for flexible CNT emitters is to realize stable
and reliable field emission performance under various bending conditions.
There have been several methods to make CNT emitters
including chemical vapor deposition, screen printing, electrophoresis, spray coating, self-assembly, and dip coating.12,19,2328 However, the above methods have several
problems for flexible applications. First, the structure and
morphology of emitters can be easily damaged under various
bending conditions, and second, weak mechanical adhesion
between emitters and substrates often occurs. In order to
overcome the above problems, we demonstrate the fabrication of flexible CNT emitters using CNT films.
In previous works on flexible CNT emitters, most studies reported the field emission properties without measuring

the emission stability from the flexible CNT emitters under


bending conditions.1622 Stable field emission is vital for
flexible CNT emitters under bending conditions. In this
work, we demonstrate the fabrication of flexible CNT emitters on a transparent plastic substrate and also evaluate the
field emission characteristics from the flexible CNT emitters
under bending conditions. In addition, we attempt to confirm
the feasibility of a flexible lamp or a flexible signage board
using such flexible CNT emitters.
Figure 1 shows schematics of the fabrication process.
Double-walled CNT (DWCNT) powder was inserted into a
0.1 wt. % sodium dodecyl sulfate solution (500 ml) and then
ultrasonically dispersed for 30 min at room temperature
using a tip type ultrasonicator, resulting in a well-dispersed
CNT suspension. The CNT suspension was filtered through a

a)

D. H. Shin and S. I. Jung contributed equally to this work.


Present address: Future Industry R&D Center, DH Holdings CO., LTD.,
705-32 Yeoksam-Dong, Kangnam-Gu, Seoul 135-080, South Korea.
c)
Author to whom correspondence should be addressed. Electronic mail:
cjlee@korea.ac.kr
b)

0003-6951/2014/105(3)/033110/5/$30.00

FIG. 1. Schematic diagram of the fabrication procedure for the flexible CNT
emitter.

105, 033110-1

C 2014 AIP Publishing LLC


V

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Shin et al.

Teflon filter membrane using vacuum suction. After drying


the filtered CNT deposit in a dry oven at 80  C, a uniform
CNT film was formed on the membrane [Fig. 1(a)]. Flexible
CNT emitter was prepared by transferring DWCNT film
onto a conductive tape [Fig. 1(b)], and then attached onto a
polyethylene terephthalate (PET) substrate [Fig. 1(c)]. The
flexible CNT emitter was baked out in a vacuum oven at
100  C for 2 h to minimize the outgassing from the sample.
A spacer (PET film) and the anode (Pt coated PET film)
were attached onto the flexible PET substrate [Fig. 1(d)].
The three parts (the cathode, the spacer and the anode) were
finally pressed and fixed by a clamp to assemble the flexible
CNT emitter. However, in order to investigate emission patterns, we used an anode which was produced by the additional deposition of a phosphor layer on the Pt film.
The field emission characteristics were evaluated in a
diode configuration at room temperature in a vacuum chamber under a pressure of less than 2  107 Torr. The gap
between the cathode and the anode was adjusted to 400 lm
using the PET film spacer. The emission area, which is determined by the exposure area via the hole in the PET spacer
(diameter of 6 mm) was 0.28 cm2. The emission current was
monitored using a Keithley 6485, and the DC power was
supplied by a high voltage source (TECHNIX SR15-P1500). We measured the field emission properties of the flexible CNT emitters under various bending conditions including curvature direction and curvature radius after several
hundred bendings. A detailed illustration for the experimental conditions is contained in supplementary Fig. S1.29

Appl. Phys. Lett. 105, 033110 (2014)

Figure 2(a) shows a scanning electron microscopy


(SEM, Hitachi S-4800) image of the as-synthesized CNTs
indicating a very high purity with network morphology, and
Fig. 2(b) indicates a transmission electron microscopy
(TEM, TECNAI F20, 200 kV) image which reveals clear
wall structures in the DWCNTs. The inset of Fig. 2(b) shows
a magnified TEM image of an individual DWCNT with a diameter of about 2 nm. Figure 2(c) shows a SEM image of the
surface of the flexible CNT emitter. Lots of CNTs are
entangled on the substrate and some protruding CNTs are
vertically aligned after mechanical treatment. This feature
means that many CNTs can take part in electron emission,
resulting in high emission current from the CNT emitter.
Figure 2(d) shows a photograph of the flexible CNT emitter
fabricated on a PET substrate. The CNT emitter shows no
cracks or damage after several hundred bendings.
Figures 2(e) and 2(f) show a Raman spectrum of the
DWCNTs obtained using Horiba Jobin-Yvon LabRAM HR800 with Ar-ion laser excitation (laser-beam wavelength:
514.5 nm). As the radial breathing mode (RBM) frequency is
inversely proportional to the diameter of CNT, we can estimate the diameter of the DWCNTs using
x 223:75=d 15;

where x is the RBM frequency (cm1) and d is the diameter


(nm) of the tube.30 The diameter distribution of the
DWCNTs is in the range of 0.92.2 nm as summarized in
supplementary Table S1,29 which well agrees with TEM
observations. The Raman spectrum of the DWCNTs shows a
weak D-band peak at 1340.9 cm1 and a strong G-band peak
at 1592.6 cm1. The small ID/IG ratio (ID/IG 0.06) indicates
a high crystalline structure of the DWCNTs with a low
degree of defects and disorder.31
When the flexible CNT emitters are bent, mechanical
strain (e) is generated on the CNT emitters. The strain generated on the flexible CNT emitters under various bending conditions can be calculated using
strain e hf hs =2r hs =2r;

FIG. 2. (a) SEM and (b) TEM images of DWCNTs. The inset shows two
graphitic layers clearly. (c) SEM image of the surface of CNT emitter. A lot
of CNTs exist and some CNTs are quasi aligned on the cathode electrode.
(d) A photograph of the flexible CNT emitter. Raman spectrum of DWCNTs
in (e) the RBM region (100300 cm1) and (f) the D- and G-band region
(10001800 cm1).

(1)

(2)

where hf, hs, and r denote the thickness of the CNT film, the
thickness of the substrate including the adhesion layer, and
curvature radius of the substrate, respectively.32 Because the
thickness of the CNT film (5 lm) is much smaller than that
of the substrate (280 lm), hf  hs, the strain can be given by
hs/2r. The CNT film used for the flexible CNT emitters has
the Youngs modulus of 460 MPa as shown in supplementary
Fig. S2.29 Consequently, mechanical stress on the flexible
CNT emitters under bending conditions can be estimated
using r e  Y where r and Y are the tensile stress and
Youngs modulus, respectively.
Figure 3 shows the resistance change rate (DR/Ro),
where DR is the difference between the current resistance
(R) and initial resistance (Ro), under various bending conditions. Electrical resistance of the flexible CNT emitters was
measured using the two-probe method with a digital multimeter (Agilent 34411A). The resistance increases up to 0.9%
under convex bending, whereas the resistance changes less
than 0.1% under concave bending. The resistance is recovered to the initial value after relaxing the strain when the

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Appl. Phys. Lett. 105, 033110 (2014)

FIG. 3. The resistance change rate of the flexible CNT emitters as a function
of curvature radius under (a) convex and (b) concave bending, respectively.

curvature is controlled between flat and curvature radius of


1.5 mm (corresponding to a strain of 9.3%). It is noteworthy
that the flexible CNT emitter shows nearly constant resistance (DR/Ro < 1%) in both bending directions until the strain
is applied up to 9.3%, which indicates a mechanical and
electrical stability of the flexible CNT emitters even under
severe bending conditions.
Figures 4(a) and 4(b) show the field emission characteristics of the flexible CNT emitters. The curvature radius of
the flexible CNT emitters was adjusted to be 10, 5, 2.5, and
0.5 mm. The flexible CNT emitters reveal very stable and
high performance field emission characteristics under various bending conditions. The flexible CNT emitter shows a
very low turn-on electric field (corresponding to an emission
current density of 0.1 lA/cm2) of 0.82 V/lm when it is flat.
The electric field to produce an emission current density of
1 mA/cm2 from the flexible CNT emitter is 1.55 V/lm, and
the maximum emission current density is about 2.0 mA/cm2
at an electric field of 1.6 V/lm. In a convex mode shown in
Fig. 4(a), the flexible CNT emitters show stable emission

FIG. 4. Field emission characteristics of the flexible CNT emitters according


to the curvature radius under (a) convex and (b) concave bending, respectively. The insets show the corresponding F-N plots. (c) Long-term field
emission stability of the flexible CNT emitters under bending condition
(convex mode, curvature radius of 10 mm) for 20 h.

current even under the severe bending conditions until the


curvature radius reaches 0.5 mm (corresponding to a strain
of 28%). The emission current becomes unstable at around
1 mA/cm2 when the flexible CNT emitters are completely
folded. In a concave mode shown in Fig. 4(b), the flexible
CNT emitters show stable emission current until the curvature radius is as small as 5 mm (corresponding to a strain of
2.8%). The stable emission behavior of the flexible CNT

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Appl. Phys. Lett. 105, 033110 (2014)

FIG. 5. Field emission patterns of the


flexible lamps using the flexible CNT
emitters under a convex mode bending.
The flexible lamps show uniform and
bright emission patterns. The emission
patterns of the flexible circular lamp
are obtained at an applied electric
fields of (a) 1.0 V/lm, (b) 1.8 V/lm,
and (c) 2.8 V/lm, respectively. (d) The
emission pattern of the flexible square
lamp is obtained at an applied electric
field of 2.8 V/lm. (Multimedia view)
[URL:
http://dx.doi.org/10.1063/
1.4891328.1][URL: http://dx.doi.org/
10.1063/1.4891328.2]

emitters using DWCNT films under several bending conditions is attributed to robust network properties due to strong
van der Waals force between DWCNTs.
However, the flexible CNT emitters suffer from frequent
arcing when the curvature radius was less than 2.5 mm under
concave bending, thus we could not obtain stable field emission properties. The relatively unstable field emission property
under concave bending is attributed to the morphological
change of the flexible CNT emitters due to the compressive
force on the CNT emitters. When the flexible CNT emitters
are under the severe concave bending conditions, several
wrinkles are generated by the compressive force, which
change electric field distributions and sometimes make electrical contacts between the anode and the emitter.
Field emission properties of flexible CNT emitters using
multi-walled CNTs (MWCNTs) were also investigated under
the identical bending conditions as shown in supplementary
Fig. S3.29 They showed slightly increasing deviation in their
emission properties compared to the flexible DWCNT emitters, which is caused by larger diameters of MWCNTs.
The insets of Figs. 4(a) and 4(b) show the corresponding
Fowler-Nordheim (F-N) plots for the flexible CNT emitters.
The field enhancement factor can be calculated by using the
F-N equation
i

 h
3
(3)
J A c2 F2 =/ exp B/2 =cF ;
where J is the emission current density, A 1.54  106
AV2 eV, B 6.83  109 eV3/2 Vm1, c is the field
enhancement factor, / is the work function, and F is the
applied electric field. Assuming the work function of CNTs
to be 5.0 eV,33 the field enhancement factor can be calculated
to be about 4091 by fitting the slope of the F-N plot (ln(J/F2)
vs. 1/F). The high value of the field enhancement factor of
the CNT emitter is attributed to the small diameter and high
aspect ratio of the DWCNTs.
We evaluated the emission current stability of the flexible CNT emitters under the bending condition using a convex mode with a curvature radius of 10 mm (corresponding

to a strain of 1.4%) as shown in Fig. 4(c). The long-term


emission stability was investigated at an initial emission current density of 0.1 mA/cm2, and the degradation of the emission current was checked under constant DC voltage for
20 h. The flexible CNT emitter shows degradation of the
emission current in the initial stages but shows the relatively
stable emission current after 4 h.
From the above results, it seems that these flexible CNT
emitters show good emission stability compared to other
results.34,35 However, fluctuation in the emission current
appears during the stability measurements under a bending
condition. Further study is necessary to get detail understanding for fluctuation of the emission current during the
long-term emission stability test.
We evaluated the feasibility of flexible lamps using the
CNT emitters under bending conditions. The flexible lamps
have either a circular shape (0.28 cm2, diameter: 6 mm) or a
square shape (15  15 mm2), which were produced via holes
in the PET spacer layer. The gap between the CNT emitter
and the anode electrode was produced using a PET film of
180 lm thickness. All the emission patterns were observed in
a vacuum chamber at a pressure of 2  107 Torr. Figure 5
shows emission patterns from the flexible lamp made using
the CNT emitters under bending conditions. As shown in
Fig. 5(a), there is no emission pattern from the flexible lamp
because electron emission at a low applied electric field of
1.0 V/lm is not sufficient to stimulate the phosphor. By
increasing the applied electric field to 1.8 V/lm, a partial
emission pattern appears from the flexible lamp due to the
enhanced electron emission as shown in Fig. 5(b). At a
higher applied electric field of 2.8 V/lm, the emission is
finally enough to produce a fully bright and uniform pattern
from the flexible lamp as shown in Fig. 5(c). The emission
pattern from a square lamp is also presented in Fig. 5(d). In
this work, flexible lamps using CNT emitters generate very
uniform and bright emission patterns under convex bending
conditions. Even though our flexible lamp displayed good
field emission performance, it was still necessary to carry out
the measurements in a vacuum chamber under continuous

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vacuum pumping and at reasonably high vacuum pressure.


Our flexible lamp using CNT emitters consists of a substrate,
a spacer and an anode electrode using PET films, which can
be prone to outgassing. For more robust and realistic flexible
CNT emitters, those parts should be replaced by other inorganic films or metallic films. Further study is under way to
develop suitable materials and processes. Nevertheless, we
consider that flexible CNT emitters using the CNT film
described herein can be important candidates for flexible
field emission devices in the future.
In summary, we have demonstrated the fabrication of the
flexible CNT emitters using CNT film and investigated the
field emission properties of the flexible CNT emitters under
various bending conditions. Our flexible CNT emitters can be
fabricated by a simple process and showed high emission performance. The flexible CNT emitters had a low turn-on electric
field of 0.82 V/lm and a maximum emission current density of
2.0 mA/cm2. The flexible CNT emitters exhibited the minimum
curvature radii of 0.5 mm and 5 mm under convex and concave
bendings, respectively. During long-term emission stability
measurements, the flexible CNT emitter showed a stable emission current while being continually bent. A flexible lamp using
the robust flexible CNT emitter showed uniform and bright
emission patterns under all bending conditions. We consider
that the high emission performance of the flexible CNT emitter
is attributed to the stable network of the CNT film under various bending conditions. We suggest that our results strongly
indicate the potential use of the flexible CNT emitters in flexible field emission applications.
This work was supported by World Class University
Project (WCU, R32-2010-000-10082-0) by the Ministry of
Education, Science, and Technology. This work was also
supported by ETRI Creative R&D program (No. 12ZF1100)
and the Korea Basic Science Institute.
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